CN103880359B - Silica alumina composite ceramics microballon prepares oil well cementing cement briquette method - Google Patents
Silica alumina composite ceramics microballon prepares oil well cementing cement briquette method Download PDFInfo
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Abstract
The invention provides silica alumina composite ceramics microballon and prepare oil well cementing cement briquette method, comprise the preparation of silica alumina composite ceramics closed pore cenosphere, batching, mixing, stirring is sized mixing, die trial, strength trial, by G level oil well cement 40 ~ 50wt%, particle diameter 13 μm of superfine cement 10 ~ 15wt%, particle diameter is the composite ceramics closed pore cenosphere 25 ~ 35wt% of 5 ~ 50 μm, flyash 5 ~ the 7wt% of loss on ignition 1.1%, purity 99.9% calcium oxide 1.5 ~ 2wt%, sodium sulfate 0.5 ~ 1.0wt% and SILICA FUME 1 ~ 3wt% mixing and stirring, with 0.5 ~ 0.6(W/C) water cement ratio stir in stirrer and size mixing 40 seconds, pour die trial into, maintenance 24 hours in the water-bath maintaining box of constant temperature 52 DEG C, 48 hours, soak 1 hour in cold water after the demoulding, carry out performance test.
Description
Technical field
The present invention relates to silica alumina composite ceramics microballon and prepare oil well cementing cement briquette method, belong to field of material technology.
Background technology
Current domestic oil well cementing light-weight additive adopts the drift pearl in flyash, and comprise heavy pearl and drift pearl at flyash, heavy pearl density is at 1.1 ~ 2.8g/cm
3between, content accounts for flyash 30 ~ 70%, and drift pearl is the glass microballon being less than water-mass density in flyash, and drift pearl mainly comprises aluminosilicate glass microballon and porous carbon granule, drift pearl after removing carbon granule mainly comprises Thin-walled Aluminum silex glass microballon, surfaces externally and internally is smooth, and volume is large, is that one is rounded, light weight, closed pore are hollow, wear-resisting, high temperature resistant, thermal conductivity is little, intensity is high, drift pearl amount accounts for 0.5 ~ 1% of flyash total amount, and aluminosilicate glass microballon is hollow spherosome.
Drift pearl wherein in flyash it be coal dust in thermal power plant boiler through 1100 ~ 1500 DEG C burning time, clayey material melts becomes microlayer model, in stove turbulent flow hot air acting under at a high speed spin, form perfectly round sial spheroid, the gases such as nitrogen, hydrogen and carbonic acid gas that burning and scission reaction produce, undergoes rapid expansion in the high temperature aluminum silicon spheroid of melting, under capillary effect, form the glass envelope of hollow, then enter flue to cool rapidly, after sclerosis, become the vitreous state cenosphere of high vacuum, i.e. fly ash float.
Flyash is put into water stir, leave standstill for some time, because drift pearl density is less than water-mass density, will swim in the water surface pulls out and dry, be and float pearl, the drift pearl in flyash is canescence, and main component is SiO
2account for 70% and AI
2o
3account for 13%, loss on ignition is 0.40% ~ 0.574%, density 0.475 ~ 0.574g/cm
3, wall thickness 1.44 ~ 5.41 μm, particle size range is mainly distributed in 147 ~ 84 μm, but the particle diameter of drift pearl is large, and ultimate compression strength is low.
In recent years, due to the impact of northern haze weather, the big-and-middle-sized thermal power generation of China adopts the desulfurization technology of environmental protection, not containing in flyash floats pearl, cause in short supply, only has the drift pearl that middle small coal power plants and arcola do not adopt desulfurization technology supply a small amount of, drift the in short supply of pearl causes price increase, and float that pearl is impure is mixed with flyash, affect cementing quality, drift pearl price per ton at least 1 ten thousand yuan, and maximum compressive strength 20MPa, so adopt composite ceramic material making cenosphere to substitute the drift pearl of flyash, not by the restriction of envrionment conditions, economic benefit is large, market outlook are good.
In reinforcing oil well field, hydrocarbon distribution is wide, and long shut-in well is more and more, and main use of long shut-in well is light weight cement well cementation, and long shut-in well mainly adopts low-density cement mortar, wants to make the density of grout at 1.0g/cm
3~ 1.5g/cm
3between, density must at 0.5g/cm for the lightening material (inorganic mineral material and organic synthesis material composition) of non-drift pearl
3~ 0.8g/cm
3between, (density of G level oil well watertight is at 3.1g/cm just to make low-density grout
3, light-weight additive density must be less than 1g/cm
3, just can configure density 1.0g/cm
3~ 1.5g/cm
3between grout, precondition is that light-weight additive addition can not exceed 40% of total amount, otherwise can affect the ultimate compression strength of cement briquette).
Different according to the well cementation degree of depth, usually the oil well of less than 2000 meters low hot-well, low temperature oil-well is cemented the well, and with highdensity grout, (, between 70 ~ 90 DEG C, namely cement slurry density is at 1.8g/cm for the temperature in oil well
3~ 1.9g/cm
3); Be middle hot-well between 2000 ~ 4000 meters, (, between 90 ~ 150 DEG C, namely cement slurry density is at 1.6g/cm for the temperature in oil well for the grout of middle temperature oil well cementing Midst density
3~ 1.7g/cm
3); And be greater than 4000 meters for hot hole, with low-density grout, (, between 150 ~ 240 DEG C, namely cement slurry density is at 1.0 g/cm for the temperature in oil well in high-temperature oil well well cementation
3~ 1.5g/cm
3).
Because land low temperature oil-well hydrocarbon resources is gradually reducing, progressively by land low temperature oil-well, landwards deep layer and bathypelagic are developed in exploitation, traditional well cementing material drift pearl can not meet the needs of deep layer high-temperature oil well, needs to employ new technology, novel process, novel material to be to meet the requirement of deep-level high pressure high-temperature oil well..
Silica alumina composite ceramic material prepares closed pore cenosphere, forms sial complex body through high temperature sintering, dioxide-containing silica up to more than 70%, have indeformable under long term high temperature condition, do not break.
Summary of the invention
The object of the invention is to overcome the existing fly ash float state of the art, the drift pearl of flyash is substituted with composite ceramics cenosphere, there is provided a kind of cost low, excellent property, the rate of change of the density of cement briquette is made to be less than 0.02, reach cementing design density, closed pore cenosphere is prepared with silica alumina composite ceramic material, through high temperature sintering, the performance index such as resistance to compression, folding strength are made to exceed the drift pearl of flyash, produce and do not affect by other conditions, composite ceramics closed pore cenosphere density range 0.5g/cm
3~ 0.8g/cm
3controlled, and then configuration 1.0g/cm
3~ 1.5g/cm
3the preparation method of oil well cementing light weight cement test block, meets the requirement of 4000 ~ 7000 meters of dark oil well long shut-in well well cementing materials.
its technical scheme is.
Comprise the preparation of silica alumina composite ceramics closed pore cenosphere, batching, mixing, stirring is sized mixing, die trial, strength trial, is characterized in that: by G level oil well cement 40 ~ 50wt%, 13 μm of superfine cement 10 ~ 15wt%, particle diameter is the silica alumina composite ceramics microballon 25 ~ 35wt% of 5 ~ 50 μm, flyash 5 ~ the 7wt% of loss on ignition 1.1%, purity 99.9% calcium oxide 1.5 ~ 2wt%, sodium sulfate 0.5 ~ 1.0wt% and SILICA FUME 1 ~ 3wt% mixes, with 0.5 ~ 0.6(W/C) water cement ratio stir in stirrer and size mixing 40 seconds, get aliquot and carry out cement slurry property test, comprise the mensuration of silica alumina composite ceramics closed pore cenosphere resistance to hydrostatic pressure intensity, cement slurry density measures, withstand voltage density test, sedimentation stability, free liquid amount of precipitation, fluid loss falls, thickening time, the liquidity scale, pours die trial (one group of two block length into, wide, high 53mm*53mm*53mm respectively), maintenance 24 hours in the water-bath maintaining box of constant temperature 52 DEG C, 48 hours, soak 1 hour in cold water after the demoulding, carry out compressive property test.
Described silica alumina composite ceramics microballon prepares oil well cementing cement briquette method, particle diameter 1 ~ 30 μm of silicon-dioxide, particle diameter 5 ~ 50 μm of aluminum oxide and binding agent are stirred by weight 92 ~ 94%:1 ~ 5%:1 ~ 3% mixed powder, at pressing machine briquetting, drying and moulding, burn 8 ~ 12 hours at 600 ~ 800 DEG C, 1000 ~ 1350 DEG C of heat preservation sinterings 12 hours, are processed into 10 ~ 50 μm of microballons by silicon-dioxide oxidation and sinter body at balling machine in a vacuum furnace.
Described silica alumina composite ceramics microballon prepares oil well cementing cement briquette method, and the weight percent of silica alumina composite ceramics microballon liquid slurry consists of: 10 ~ 50 μm of silica alumina composite ceramics microballons 70 ~ 80wt%: water 20 ~ 30wt%.
Described silica alumina composite ceramics microballon prepares oil well cementing cement briquette method, and in silica alumina composite ceramics microballon liquid slurry, add whipping agent is one in light calcium carbonate, potassium sulfate or sodium sulfate, and the concentration of use is 1 ~ 3g/L.
Described silica alumina composite ceramics microballon prepares oil well cementing cement briquette method, silica alumina composite ceramics microballon liquid is starched abundant agitation and filtration, adopt high pressure spraying high speed centrifugation rotary spraying technique, form microballoon, expansion temperature that four district's electric furnaces dewater 800 ~ 850 DEG C, dry sintering temperature 1400 ~ 1600 DEG C, melt surface temperature 1700 ~ 1800 DEG C, become bulb temperature 1400 ~ 1500 DEG C, obtain 10 ~ 50 μm of silica alumina composite ceramics closed pore cenospheres through classification.
Described silica alumina composite ceramics microballon prepares oil well cementing cement briquette method, and silica alumina composite ceramics closed pore cenosphere its floatability is greater than 95%.
Described silica alumina composite ceramics microballon prepares oil well cementing cement briquette method, and the cement briquette 8 hours ultimate compression strength of preparation is greater than 15MPa, and within 24 hours, ultimate compression strength is greater than 20MPa.
Described silica alumina composite ceramics microballon prepares oil well cementing cement briquette method, and the fluid loss that falls of cement stone is less than 50ml/30min.
Described silica alumina composite ceramics microballon prepares oil well cementing cement briquette method, and cement briquette rate of change of the density is less than 0.02.
Described silica alumina composite ceramics microballon prepares oil well cementing cement briquette method, silica alumina composite ceramics closed pore cenosphere resistance to hydrostatic pressure intensity 60 ~ 100MPa.
The present invention has the following advantages.
1, can change the dependence to flyash floating bead in long-term well cementation, adopt the lightening material of composite ceramic material making needed for oil well cementing, the production technique such as density, wall thickness, sintering temperature of ceramic fine bead can control.
2, this technical matters is advanced, and technology maturation, product performance are stable, and production cost is low, and output is high, and performance is good, opens well cementation synthesis virgin material new way.
3
,silica alumina composite ceramics bead density can be controlled in 0.5g/cm
3~ 0.8g/cm
3add the early strength that 13 μm of superfine cements can increase Behavior of Hardened Cement Paste test block, according to piling up the theoretical space added between SILICA FUME filler particles, increase dioxide-containing silica and cement slurry suspension stability machine Behavior of Hardened Cement Paste high temperature resistance, G level oil well cement, superfine cement, ceramic fine bead have greater activity through more than 1000 DEG C high temperature sinterings, hydration reaction is fast, can form jelly, can improve early strength.
4
,utilize vertical four district high temperature Cheng Zhulu, adopt high pressure spraying high speed centrifugation rotary spraying technique, spraying sheet aperture decides granular size, body of heater is entered after liquid is fully atomized, drop is at breathing space expanded by heating, and expanding volume is relevant with expansion temperature and density of foaming agent, then through sintering, melting, last balling-up, prevent knot wall from adopting thermal cycling air-bleed system to improve output, blower fan adopts speed control by frequency variation blower fan.
5, because silica alumina composite ceramics microballon particle diameter is little, and the avidity of grout is strong, and grout stability is strong.
6, spheronization techniques is that material is blown afloat by blower fan, motion phase mutual friction between material with material, forms circular or subcircular particle.
Embodiment.
Embodiment 1.
(1) 1. the preparation of silica alumina composite ceramics closed pore cenosphere is prepared burden and is fired: by particle diameter 1 ~ 10 μm of silicon-dioxide, particle diameter 5 ~ 20 μm of aluminum oxide and binding agent stir by 92wt%:5wt%:3wt% mixed powder, at pressing machine briquetting, drying and moulding, burn 10 hours at 600 DEG C, heat preservation sintering 12 hours in 1150 DEG C of vacuum ovens, silica alumina sintered compact is processed into 10 ~ 20 μm of microballons at balling machine, 2. dosing: 10 ~ 20 μm of silica alumina composite ceramics microballons 75wt%: water 25wt%, light calcium carbonate whipping agent is added in liquid slurry, concentration is 1g/L, 3. filter: by macrobead and Impurity removal, 4. fire: adopt high pressure spraying high speed centrifugation rotary spraying technique, form microballoon, on vertical four district's electric furnaces, dehydration is expanded, dry sintering, melt surface, balling-up, through dehydration expansion temperature 800 DEG C on four district's electric furnaces, dry sintering temperature at 1400 DEG C, melt surface 1700 DEG C, become bulb temperature 1400 DEG C, clean classification through wind-force and obtain 5 ~ 15 μm of silica alumina composite ceramics closed pore cenospheres.
(2) 5 ~ 15 μm of silica alumina composite ceramics closed pore hollow ceramic microspheres 50g are got, put into the beaker filling water, 1 minute is stirred with glass stick, leave standstill 5 minutes, observe the suspended state of silica alumina composite ceramics closed pore cenosphere grain in beaker, drift pearl in beaker and heavy pearl are taken out oven dry respectively weigh, calculate its floatability.
(3) the composite ceramics closed pore cenosphere grain 100g of 5 ~ 15 μm is got, put into hydrostaticpressure instrument, water enters pressure chamber by hydraulic pamp through capillary pressure pipe, the percentage of damage of drift pearl increases along with the increase of hydrostaticpressure, write down hydrostaticpressure force value, off-test, take out pressure chamber, sample compound being floated pearl is poured into and is filled in the beaker of water, by floating in beaker for intact drift pearl, drift pearl of breaking sinks to the bottom of beaker, the drift pearl in beaker and heavy pearl is taken out oven dry respectively and weighs, calculate percentage of damage and static-pressure-resisting, 2 ~ 3 times can be repeated.
(4) 5 ~ 15 μm of silica alumina composite ceramics closed pore cenosphere size distribution are analyzed with laser particle size analyzer, wind-force is cleaned classification to obtain silica alumina composite ceramics closed pore cenosphere and take 50g and pour beaker into and add 100g water, stir with glass stick, pour in laser particle size analyzer test trough, observed and recorded sample particle diameter distributes.
(5) low density oil well cementing cement briquette batching: silica alumina composite ceramics closed pore cenosphere 35wt%, the flyash 5wt% of loss on ignition 1.1%, purity 99.9% calcium oxide 1.5wt%, the sodium sulfate 0.5wt% and SILICA FUME 3wt% that by G level oil well cement 40wt%, 13 μm of superfine cement 15wt%, particle diameter are 5 ~ 15 μm.
(6) mix: get G level oil well cement 40wt%, 13 μm of superfine cement 15wt%, particle diameter be 5 ~ 15 μm silica alumina composite ceramics closed pore cenosphere 35wt%, loss on ignition 1.1% flyash 5wt%, purity 99.9% calcium oxide 1.5wt%, that sodium sulfate 0.5wt% and SILICA FUME 3wt% puts into stirrer for mixing is even.
(7) get in (6) that to mix sample a little, pour in beaker, by 0.5(W/C) water cement ratio modulation grout, stir with glass stick, pour in mud scale and weigh density.
(8) at temperature 28 DEG C ± 1 DEG C, with 0.5(W/C) water cement ratio pour corrugation agitator into, under even low speed, all mixed in 20 seconds, then build the lid of agitator, continue to stir 40 seconds under the speed of 4000r/min, leave standstill 5 minutes and observe grout homogeneity.
(9) poured into by the grout be stirred in the die trial of a group two pieces, the specification of die trial is long 53mm, wide 53mm height 53mm.
(10) observe weigh and record free liquid amount of precipitation, fall fluid loss, the thickening time, the liquidity scale.
(11) maintenance 24 hours in the water-bath maintaining box of constant temperature 52 DEG C, soaks 1 hour after the demoulding in cold water, carries out ultimate compression strength and folding strength test and rate of change of the density experiment by the regulation of GB GB/T 177.
(12) maintenance 48 hours in the water-bath maintaining box of constant temperature 52 DEG C, soaks 1 hour after the demoulding in cold water, carries out ultimate compression strength and folding strength test and rate of change of the density experiment by the regulation of GB GB/T 177.
Embodiment 2.
(1) 1. the preparation of silica alumina composite ceramics closed pore cenosphere is prepared burden and is fired: by particle diameter 10 ~ 20 μm of silicon-dioxide, particle diameter 20 ~ 35 μm of aluminum oxide and binding agent stir by 95wt%:3wt%:2wt% mixed powder, at pressing machine briquetting, drying and moulding, burn 10 hours at 700 DEG C, heat preservation sintering 12 hours in 1250 DEG C of vacuum ovens, silica alumina sintered compact is processed into 20 ~ 30 μm of microballoons at balling machine, 2. dosing: 20 ~ 30 μm of silica alumina composite ceramics microballons 72wt%: water 28wt%, lightweight potassium sulfate whipping agent is added in liquid slurry, concentration is 2g/L, 3. filter: by macrobead and Impurity removal, 4. fire: adopt high pressure spraying high speed centrifugation rotary spraying technique, form microballoon, on vertical four district's electric furnaces, dehydration is expanded, dry sintering, melt surface, balling-up, through dehydration expansion temperature 820 DEG C on four district's electric furnaces, dry sintering temperature at 1500 DEG C, melt surface temperature 1750 DEG C, become bulb temperature 1450 DEG C, clean classification through wind-force and obtain 20 ~ 30 μm of silica alumina composite ceramics closed pore cenospheres.
(2) 20 ~ 30 μm of silica alumina composite ceramics closed pore cenosphere 50g are got, put into the beaker filling water, 1 minute is stirred with glass stick, leave standstill 5 minutes, observe the suspended state of silica alumina composite ceramics closed pore cenosphere in beaker, drift pearl in beaker and heavy pearl are taken out oven dry respectively weigh, calculate its floatability.
(3) the silica alumina composite ceramics closed pore cenosphere 100g of 20 ~ 30 μm is got, put into hydrostaticpressure instrument, water enters pressure chamber by hydraulic pamp through capillary pressure pipe, the percentage of damage of drift pearl increases along with the increase of hydrostaticpressure, write down hydrostaticpressure force value, off-test, take out pressure chamber, being poured into by the sample of drift pearl fills in the beaker of water, by floating in beaker for intact drift pearl, drift pearl of breaking sinks to the bottom of beaker, the drift pearl in beaker and heavy pearl is taken out oven dry respectively and weighs, calculate percentage of damage and static-pressure-resisting, 2 ~ 3 times can be repeated.
(4) 20 ~ 30 μm of silica alumina compound closed pore hollow ceramic microspheres size distribution are analyzed with laser particle size analyzer, wind-force is cleaned classification to obtain silica alumina composite ceramics closed pore cenosphere and take 50g and pour beaker into and add 100g water, stir with glass stick, pour in laser particle size analyzer test trough, observed and recorded sample particle diameter distributes.
(5) low density oil well cementing cement briquette batching: get G level oil well cement 45wt%, 13 μm of superfine cement 15wt%, particle diameter is silica alumina composite ceramics closed pore cenosphere 30wt%, the flyash 6wt% of loss on ignition 1.1%, purity 99.9% calcium oxide 2wt%, the sodium sulfate 1wt% and SILICA FUME 1wt% of 20 ~ 30 μm.
(6) mix: get G level oil well cement 45wt%, 13 μm of superfine cement 15wt%, particle diameter be 20 ~ 30 μm silica alumina composite ceramics closed pore cenosphere 30wt%, loss on ignition 1.1% flyash 6wt%, purity 99.9% calcium oxide 2wt%, that sodium sulfate 1wt% and SILICA FUME 1wt% puts into stirrer for mixing is even.
(7) get in (6) and mix sample a little, pour in beaker, by the water cement ratio modulation grout of 0.6, stir with glass stick, pour in mud scale and weigh density.
(8) at temperature 28 DEG C ± 1 DEG C, with 0.6(W/C) water cement ratio pour corrugation agitator into, under even low speed, all mixed in 20 seconds, then build the lid of agitator, continue to stir 40 seconds under the speed of 4000r/min, leave standstill 5 minutes and observe grout homogeneity.
(9) poured into by the grout be stirred in the die trial of a group two pieces, the specification of die trial is long 53mm, wide 53mm height 53mm.
(10) observed and recorded free liquid amount of precipitation, fluid loss, thickening time, the liquidity scale fall.
(11) maintenance 24 hours in the water-bath maintaining box of constant temperature 52 DEG C, soaks 1 hour after the demoulding in cold water, carries out ultimate compression strength and folding strength test and rate of change of the density experiment by the regulation of GB GB/T 177.
(12) maintenance 48 hours in the water-bath maintaining box of constant temperature 52 DEG C, soaks 1 hour after the demoulding in cold water, carries out ultimate compression strength and folding strength test and rate of change of the density experiment by the regulation of GB GB/T 177.
Embodiment 3.
(1) 1. the preparation of silica alumina composite ceramics closed pore cenosphere is prepared burden and is fired: by particle diameter 20 ~ 30 μm of silicon-dioxide, particle diameter 35 ~ 50 μm of aluminum oxide and binding agent stir by 94wt%:5wt%:1wt% mixed powder, at pressing machine briquetting, drying and moulding, burn 10 hours at 800 DEG C, heat preservation sintering 12 hours in 1350 DEG C of vacuum ovens, silica alumina sintered compact is processed into 40 ~ 50 μm of microballons at balling machine, 2. dosing: 40 ~ 50 μm of silica alumina composite ceramics microballons press 80wt%: water 20wt%, lightweight sodium sulfate whipping agent is added in liquid slurry, concentration is 3g/L, 3. filter: by macrobead and Impurity removal, 4. fire: adopt high pressure spraying high speed centrifugation rotary spraying technique, form microballoon, on vertical four district's electric furnaces, dehydration is expanded, dry sintering, melt surface, balling-up, through dehydration expansion 850 DEG C on four district's electric furnaces, dry sintering temperature at 1600 DEG C, melt surface temperature 1800 DEG C, become bulb temperature 1500 DEG C, clean classification through wind-force and obtain 35 ~ 50 μm of silica alumina composite ceramics closed pore cenospheres.
(2) 35 ~ 50 μm of silica alumina composite ceramics closed pore cenosphere 50g are got, put into the beaker filling water, 1 minute is stirred with glass stick, leave standstill 5 minutes, observe the suspended state of silica alumina composite ceramics closed pore cenosphere in beaker, drift pearl in beaker and heavy pearl are taken out oven dry respectively weigh, calculate its floatability.
(3) the silica alumina composite ceramics closed pore cenosphere 100g of 35 ~ 50 μm is got, put into hydrostaticpressure instrument, water enters pressure chamber by hydraulic pamp through capillary pressure pipe, the percentage of damage of drift pearl increases along with the increase of hydrostaticpressure, write down hydrostaticpressure force value, off-test, take out pressure chamber, being poured into by the sample of drift pearl fills in the beaker of water, by floating in beaker for intact drift pearl, drift pearl of breaking sinks to the bottom of beaker, the drift pearl in beaker and heavy pearl is taken out oven dry respectively and weighs, calculate percentage of damage and static-pressure-resisting.
(4) 35 ~ 50 μm of silica alumina composite ceramics closed pore cenosphere size distribution are analyzed with laser particle size analyzer, wind-force is cleaned classification to obtain silica alumina composite ceramics closed pore cenosphere and claim 50g to pour beaker into add 100g water, stir with glass stick, pour in laser particle size analyzer test trough, observed and recorded sample particle diameter distributes.
(5) low density oil well cementing cement briquette batching: by getting G level oil well cement 45wt%, 13 μm of superfine cement 12wt%, particle diameter is silica alumina composite ceramics closed pore cenosphere 33wt%, the flyash 7wt% of loss on ignition 1.1%, purity 99.9% calcium oxide 1.5wt%, the sodium sulfate 0.5wt% and SILICA FUME 1wt% of 35 ~ 50 μm.
(6) mix: get G level oil well cement 45wt%, 13 μm of superfine cement 12wt%, particle diameter be 35 ~ 50 μm silica alumina composite ceramics closed pore cenosphere 33wt%, loss on ignition 1.1% flyash 7wt%, purity 99.9% calcium oxide 1.5wt%, that sodium sulfate 0.5wt% and SILICA FUME 1wt% puts into stirrer for mixing is even.
(7) get in (6) that to mix sample a little, pour in beaker, by 0.55(W/C) water cement ratio modulation grout, stir with glass stick, pour in mud scale and weigh density,
(8) at temperature 28 DEG C ± 1 DEG C, with 0.55(W/C) water cement ratio pour corrugation agitator into, under even low speed, all mixed in 20 seconds, then build the lid of agitator, continue to stir 40 seconds under the speed of 4000r/min, leave standstill 5 minutes and observe grout homogeneity.
(9) poured into by the grout be stirred in the die trial of a group two pieces, the specification of die trial is long 53mm, wide 53mm height 53mm.
(10) observed and recorded free liquid amount of precipitation, fluid loss, thickening time, the liquidity scale fall.
(11) maintenance 24 hours in the water-bath maintaining box of constant temperature 52 DEG C, soaks 1 hour after the demoulding in cold water, carries out ultimate compression strength and folding strength test and rate of change of the density experiment by the regulation of GB GB/T 177.
(12) maintenance 48 hours in the water-bath maintaining box of constant temperature 52 DEG C, soaks 1 hour after the demoulding in cold water, carries out ultimate compression strength and folding strength test and rate of change of the density experiment by the regulation of GB GB/T 177.
Note: G level oil well cement is Qi Yin cement mill, Shandong, the prosperous sub-calcium industry of purity 99.9% calcium oxide Shandong Zibo, the flyash Huaneng Group Xin Dian power plant of loss on ignition 1.1%.
Claims (6)
1. silica alumina composite ceramics microballon prepares oil well cementing cement briquette method, comprise the preparation of silica alumina composite ceramics closed pore cenosphere, batching, mixing, stirring is sized mixing, die trial, strength trial, it is characterized in that: by particle diameter 1 ~ 30 μm of silicon-dioxide, particle diameter 5 ~ 50 μm of aluminum oxide and binding agent stir by weight 92 ~ 94wt%:1 ~ 5wt%:1 ~ 3wt% mixed powder, above constituent mass per-cent sum is 100%, at pressing machine briquetting, drying and moulding, burn 8 ~ 12 hours at 600 ~ 800 DEG C, 1000 ~ 1350 DEG C of heat preservation sinterings 12 hours in a vacuum furnace, silicon-dioxide oxidation and sinter body is processed into 10 ~ 50 μm of microballons at balling machine, the weight percent of silica alumina composite ceramics microballon liquid slurry consists of 10 ~ 50 μm of silica alumina composite ceramics microballons 70 ~ 80wt%: water 20 ~ 30wt%, in silica alumina composite ceramics microballon liquid slurry, add whipping agent is one in light calcium carbonate, potassium sulfate or sodium sulfate, and the concentration of use is 1 ~ 3g/L, silica alumina composite ceramics microballon liquid is starched abundant agitation and filtration, adopt high pressure spraying high speed centrifugation rotary spraying technique, form microballoon, expansion temperature that four district's electric furnaces dewater 800 ~ 850 DEG C, dry sintering temperature 1400 ~ 1600 DEG C, melt surface temperature 1700 ~ 1800 DEG C, become bulb temperature 1400 ~ 1500 DEG C, obtain 10 ~ 50 μm of silica alumina composite ceramics closed pore cenospheres through classification, by G level oil well cement 40 ~ 50wt%, particle diameter 13 μm of superfine cement 10 ~ 15wt%, particle diameter is the silica alumina composite ceramics closed pore cenosphere 25 ~ 35wt% of 5 ~ 50 μm, flyash 5 ~ the 7wt% of loss on ignition 1.1%, purity 99.9% calcium oxide 1.5 ~ 2wt%, sodium sulfate 0.5 ~ 1.0wt% and SILICA FUME 1 ~ 3wt% mixes, water cement ratio with 0.5 ~ 0.6 stirs in stirrer sizes mixing 40 seconds, get aliquot and carry out cement slurry property test, comprise the mensuration of silica alumina composite ceramics closed pore cenosphere resistance to hydrostatic pressure intensity, cement slurry density measures, withstand voltage density test, sedimentation stability, free liquid amount of precipitation, fluid loss falls, thickening time, the liquidity scale, pour one group of two block length into, wide, height is respectively in 53mm*53mm*53mm die trial, difference maintenance 24 hours in the water-bath maintaining box of constant temperature 52 DEG C, 48 hours, soak 1 hour in cold water after the demoulding, carry out compressive property test.
2. silica alumina composite ceramics microballon according to claim 1 prepares oil well cementing cement briquette method, it is characterized in that: silica alumina composite ceramics closed pore cenosphere its floatability is greater than 95%.
3. silica alumina composite ceramics microballon according to claim 1 prepares oil well cementing cement briquette method, it is characterized in that: the cement briquette 8 hours ultimate compression strength of preparation is greater than 15MPa, and within 24 hours, ultimate compression strength is greater than 20MPa.
4. silica alumina composite ceramics microballon according to claim 1 prepares oil well cementing cement briquette method, it is characterized in that: the fluid loss that falls of cement briquette is less than 50ml/30min.
5. silica alumina composite ceramics microballon according to claim 1 prepares oil well cementing cement briquette method, it is characterized in that: cement briquette rate of change of the density is less than 0.02.
6. silica alumina composite ceramics microballon according to claim 1 prepares oil well cementing cement briquette method, it is characterized in that: silica alumina composite ceramics closed pore cenosphere resistance to hydrostatic pressure intensity 60 ~ 100MPa.
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| CN104058760B (en) * | 2014-07-01 | 2016-01-20 | 辽宁科技大学 | A kind of method of synthetic drift pearl |
| CN104592964A (en) * | 2015-01-07 | 2015-05-06 | 山东理工大学 | Method for preparing oil well cementing test block resistant to high temperatures and high pressures from silicozirconium ceramic microspheres |
| CN105926784B (en) * | 2016-05-04 | 2018-04-10 | 同成七彩建筑科技有限公司 | Thermal insulation concrete wall construction method |
| CN107748248A (en) * | 2017-11-21 | 2018-03-02 | 淄博职业学院 | Anti-pressure glass fibre vermiculite prepares the well cementation test block performance test of oil well water-impervious |
| CN108007735A (en) * | 2017-11-21 | 2018-05-08 | 淄博职业学院 | Intumescent ceramic fibre Copper Ores prepare oil well antiseepage well cementation test block performance test |
| CN107976532A (en) * | 2017-11-21 | 2018-05-01 | 淄博职业学院 | Aluminium wollastonite ceramics microballon prepares the performance test of oil well anti-gas-leak well cementation test block |
| CN108037272A (en) * | 2017-11-21 | 2018-05-15 | 淄博职业学院 | Aluminium ore soil ceramic fine bead prepares the test method of oil well anti-gas-leak well cementation test block performance |
| CN108007742A (en) * | 2017-11-21 | 2018-05-08 | 淄博职业学院 | High air-resistance type glass fibre aluminium ore slag prepares oil well antiseepage well cementation test block performance test |
| CN107860899A (en) * | 2017-11-21 | 2018-03-30 | 淄博职业学院 | Modified silicon aluminum ceramic microspheres prepare the well cementation test block of oil well anti-gas-leak and performance test |
| CN115849798A (en) * | 2023-03-01 | 2023-03-28 | 成都理工大学 | High-strength temporary plugging cement for geothermal well based on surface modified ceramic and preparation method thereof |
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| CN103319129A (en) * | 2013-06-27 | 2013-09-25 | 东南大学 | Ecological nanoparticle reinforced cement based composite material and preparation method thereof |
| CN103467016A (en) * | 2013-09-02 | 2013-12-25 | 山东理工大学 | Preparation method for preparing low-density oil well cement test block from composite ceramic microbeads |
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| CN103319129A (en) * | 2013-06-27 | 2013-09-25 | 东南大学 | Ecological nanoparticle reinforced cement based composite material and preparation method thereof |
| CN103467016A (en) * | 2013-09-02 | 2013-12-25 | 山东理工大学 | Preparation method for preparing low-density oil well cement test block from composite ceramic microbeads |
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